RU2015105187A - METHOD FOR USING POLYREA NANOSIZED PARTICLES AS OPERATING CHARACTERISTICS IN THE COMPOSITION OF POLYURETHANE MATERIALS - Google Patents

METHOD FOR USING POLYREA NANOSIZED PARTICLES AS OPERATING CHARACTERISTICS IN THE COMPOSITION OF POLYURETHANE MATERIALS Download PDF

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RU2015105187A
RU2015105187A RU2015105187A RU2015105187A RU2015105187A RU 2015105187 A RU2015105187 A RU 2015105187A RU 2015105187 A RU2015105187 A RU 2015105187A RU 2015105187 A RU2015105187 A RU 2015105187A RU 2015105187 A RU2015105187 A RU 2015105187A
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range
component
composition
particles
polyurea particles
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RU2015105187A
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RU2604739C2 (en
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Стив Андре ВАУТТЕРС
Кристофер Иан ЛИНДСЕЙ
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Хантсмэн Интернэшнл Ллс
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    • C08J2375/08—Polyurethanes from polyethers

Abstract

1. Способ получения наноразмерных полимочевинных частиц или дисперсий указанных полимочевинных частиц, характеризующихся размерностью эквивалентного диаметра, составляющей в диапазоне 50 нм - 700 нм, узким распределением частиц по размерам по величине эквивалентного диаметра, при котором относительный разброс d-d/d<3, предпочтительно <2,5, соотношением количества мочевинных связей и количества уретановых в составе указываемых частиц, составляющим, по меньшей мере, 90:10, более предпочтительно 99:1, а также температурой стеклования (Tg), составляющей >100°С, предпочтительно Tg>120°С, более предпочтительно составляющей >150°С, измеряемой в ходе второго цикла нагревания после нагрева до температуры >220°С при скорости 20°С в минуту с использованием метода дифференциальной сканирующей калориметрии, при этом указанный способ включает в себя такие стадии, как:- совмещение реакционноспособного по отношению к изоцианатам моноаминного компонента с полиизоцианатным компонентом с образованием тем самым модифицированного мочевиной полиизоцианатного компонента, необязательно растворенного в растворителе, а затем- добавление указанного модифицированного мочевиной полиизоцианатного компонента к диаминному компоненту с образованием тем самым полимочевинных частиц, необязательно диспергированных в среде растворителя,отличающийся тем, что диаминный компонент выбирают из компонентов, отвечающих структурной формуле [2]:HN-(A)-NH[2],в которой- q представляет собой целое число меньше 4,- Aможет представлять собой С2, С3 или разветвленную С3 группу,- Aможет представлять собой одну или более ароматические группы, предпочтительно 1-4 ароматические группы,- Aможет представлять собой1. A method for producing nanosized polyurea particles or dispersions of said polyurea particles characterized by a dimension of equivalent diameter ranging from 50 nm to 700 nm, a narrow particle size distribution by equivalent diameter, in which the relative scatter dd / d <3, preferably <2 , 5, by the ratio of the number of urea bonds and the amount of urethane in the composition of the indicated particles, comprising at least 90:10, more preferably 99: 1, and also the glass transition temperature (Tg), constituting d> 100 ° C, preferably Tg> 120 ° C, more preferably component> 150 ° C, measured during the second heating cycle after heating to> 220 ° C at a speed of 20 ° C per minute using the differential scanning calorimetry method, at this method includes steps such as: - combining a monoamine component reactive with respect to isocyanates with a polyisocyanate component, thereby forming a urea-modified polyisocyanate component, optionally dissolved in a solution then adding the specified urea-modified polyisocyanate component to the diamine component, thereby forming polyurea particles, optionally dispersed in the solvent medium, characterized in that the diamine component is selected from components corresponding to the structural formula [2]: HN- (A) - NH [2] in which - q is an integer less than 4, - A can be a C2, C3 or branched C3 group, - A can be one or more aromatic groups, preferably 1-4 aromatically e groups - A may be

Claims (12)

1. Способ получения наноразмерных полимочевинных частиц или дисперсий указанных полимочевинных частиц, характеризующихся размерностью эквивалентного диаметра, составляющей в диапазоне 50 нм - 700 нм, узким распределением частиц по размерам по величине эквивалентного диаметра, при котором относительный разброс d90-d10/d50<3, предпочтительно <2,5, соотношением количества мочевинных связей и количества уретановых в составе указываемых частиц, составляющим, по меньшей мере, 90:10, более предпочтительно 99:1, а также температурой стеклования (Tg), составляющей >100°С, предпочтительно Tg>120°С, более предпочтительно составляющей >150°С, измеряемой в ходе второго цикла нагревания после нагрева до температуры >220°С при скорости 20°С в минуту с использованием метода дифференциальной сканирующей калориметрии, при этом указанный способ включает в себя такие стадии, как:1. A method for producing nanosized polyurea particles or dispersions of said polyurea particles characterized by a dimension of equivalent diameter in the range of 50 nm to 700 nm, a narrow particle size distribution by the size of the equivalent diameter, at which the relative dispersion is d 90 -d 10 / d 50 < 3, preferably <2.5, the ratio of the number of urea bonds and the amount of urethane in the composition of the indicated particles, comprising at least 90:10, more preferably 99: 1, as well as the glass transition temperature (Tg), comp which is> 100 ° C, preferably Tg> 120 ° C, more preferably component> 150 ° C, measured during the second heating cycle after heating to> 220 ° C at a speed of 20 ° C per minute using the differential scanning calorimetry method, at this method includes stages such as: - совмещение реакционноспособного по отношению к изоцианатам моноаминного компонента с полиизоцианатным компонентом с образованием тем самым модифицированного мочевиной полиизоцианатного компонента, необязательно растворенного в растворителе, а затем- combining a monoamine component reactive with isocyanates with a polyisocyanate component to thereby form a urea-modified polyisocyanate component, optionally dissolved in a solvent, and then - добавление указанного модифицированного мочевиной полиизоцианатного компонента к диаминному компоненту с образованием тем самым полимочевинных частиц, необязательно диспергированных в среде растворителя,- adding said urea-modified polyisocyanate component to the diamine component, thereby forming polyurea particles, optionally dispersed in a solvent medium, отличающийся тем, что диаминный компонент выбирают из компонентов, отвечающих структурной формуле [2]:characterized in that the diamine component is selected from components corresponding to the structural formula [2]: H2N-(A5)q-NH2 [2],H 2 N- (A 5 ) q —NH 2 [2], в которойwherein - q представляет собой целое число меньше 4,- q is an integer less than 4, - A5 может представлять собой С2, С3 или разветвленную С3 группу,- A 5 may be a C2, C3 or branched C3 group, - A5 может представлять собой одну или более ароматические группы, предпочтительно 1-4 ароматические группы,- A 5 may represent one or more aromatic groups, preferably 1-4 aromatic groups, - A5 может представлять собой арил-алифатическую группу, в которой алифатическая часть представляет собой C1-C6, и дополнительно содержит в своем составе 1-4 ароматические группы,- A 5 may be an aryl-aliphatic group, in which the aliphatic part is C1-C6, and additionally contains 1-4 aromatic groups, - A5 может представлять собой С3-С15 циклоалифатическую группу, а также- A 5 may be a C3-C15 cycloaliphatic group, and - A5 может дополнительно содержать в своем составе простую эфирную функциональную группу и/или одну или несколько NH-групп.- A 5 may additionally contain in its composition a simple ether functional group and / or one or more NH-groups. 2. Способ в соответствии с п. 1, в котором диаминный компонент выбирают из этилендиамина, гексаметилендиамина, трициклодекандиамина, неопентандиамина, диэтилтолуолдиамина, 4-метил-1,2-фенилендиамина.2. The method according to claim 1, wherein the diamine component is selected from ethylene diamine, hexamethylene diamine, tricyclodecandiamine, neopentanediamine, diethyl toluene diamine, 4-methyl-1,2-phenylenediamine. 3. Способ в соответствии с любым из пп. 1 и 2, в котором моноаминные компоненты представляют собой алкилполиоксиалкилмоноамины, описываемые следующей общей структурной формулой [1]:3. The method in accordance with any of paragraphs. 1 and 2, in which the monoamine components are alkylpolyoxyalkylmonoamines described by the following general structural formula [1]: A1-(OA2)n-(OA3)m-(OA4)p-NH2 [1],A 1 - (OA 2 ) n - (OA 3 ) m - (OA 4 ) p -NH 2 [1], в которойwherein - A1 представляет собой углеродную С1-С6 цепь, наиболее предпочтительно CH3-функциональную группу,- A 1 represents a carbon C1-C6 chain, most preferably a CH 3 functional group, - А2, А3 и А4, как правило, представляют собой взаимно-различные углеродные С1-С6 цепи, в наибольшей степени предпочтительно, по меньшей мере, одна из которых является углеродной C2-цепью, по меньшей мере, одна из которых является разветвленной углеродной С3-цепью, и, по меньшей мере, одна из которых является неразветвленной углеродной С3-цепью,- A 2 , A 3 and A 4 , as a rule, are mutually different carbon C1-C6 chains, most preferably at least one of which is a carbon C2 chain, at least one of which is branched carbon C3 chain, and at least one of which is an unbranched carbon C3 chain, - индексы n, m и p независимо являются положительными целыми числами, причем, по меньшей мере, одно из них имеет значение больше нуля.- indices n, m and p are independently positive integers, and at least one of them has a value greater than zero. 4. Способ в соответствии с любым из пп. 1 и 2, в котором моноаминные компоненты представляют собой алкилполиоксиалкилмоноамины, описываемые следующей общей структурной формулой [1]:4. The method in accordance with any one of paragraphs. 1 and 2, in which the monoamine components are alkylpolyoxyalkylmonoamines described by the following general structural formula [1]: A1-(OA2)n-(OA3)m-(OA4)p-NH2 [1],A 1 - (OA 2 ) n - (OA 3 ) m - (OA 4 ) p -NH 2 [1], в которойwherein A1 представляет собой группу C9H19-Ø-, в которой Ø представляет собой ароматическое С6-кольцо.A 1 represents a group C 9 H 19 -Ø-, in which Ø represents an aromatic C6 ring. 5. Способ в соответствии с любым из пп. 1 и 2, в котором отношение изоцианатных функциональных групп в составе полиизоцианатного компонента, рассчитанное на общее количество реакционноспособных атомов водорода в составе моноаминного компонента и диаминного компонента, предпочтительно составляет в диапазоне 80-120, более предпочтительно составляет в диапазоне 90-110, наиболее предпочтительно составляет в диапазоне 99-101.5. The method in accordance with any of paragraphs. 1 and 2, in which the ratio of isocyanate functional groups in the composition of the polyisocyanate component, calculated on the total number of reactive hydrogen atoms in the composition of the monoamine component and the diamine component, is preferably in the range of 80-120, more preferably in the range of 90-110, most preferably is in the range of 99-101. 6. Способ в соответствии с любым из пп. 1 и 2, в котором соотношение числа изоцианатных функциональных групп в составе полиизоцианатного компонента и числа первичных и вторичных аминогрупп в составе моноаминного компонента предпочтительно составляет в диапазоне 1,6-120, более предпочтительно составляет в диапазоне 10-70 и наиболее предпочтительно составляет в диапазоне 20-40.6. The method in accordance with any of paragraphs. 1 and 2, in which the ratio of the number of isocyanate functional groups in the composition of the polyisocyanate component and the number of primary and secondary amino groups in the monoamine component is preferably in the range of 1.6-120, more preferably in the range of 10-70, and most preferably in the range of 20 -40. 7. Способ в соответствии с любым из пп. 1 и 2, в котором подходящие растворители включают в себя кетоны, такие как ацетон, тетрагидрофуран (ТГФ), толуол, …, и полиолы, которые являются реакционноспособными по отношению к изоцианатам при температуре выше 60°С.7. The method in accordance with any one of paragraphs. 1 and 2, in which suitable solvents include ketones, such as acetone, tetrahydrofuran (THF), toluene, ..., and polyols that are reactive with isocyanates at temperatures above 60 ° C. 8. Способ в соответствии с любым из пп. 1 и 2, в котором дисперсия полимочевинных частиц содержит в диапазоне 0,5% масс - 50% масс частиц в среде удовлетворяющего требованиям растворителя, предпочтительно содержит в диапазоне 1-30% масс, более предпочтительно содержит в диапазоне 5-20% масс.8. The method in accordance with any of paragraphs. 1 and 2, in which the dispersion of polyurea particles contains in the range of 0.5% to 50% by weight of the particles in an environment that meets the requirements of the solvent, preferably contains in the range of 1-30% of the mass, more preferably contains in the range of 5-20% of the mass. 9. Способ образования эластичного пенополиуретана, характеризующегося величиной плотности при свободном подъеме, составляющей менее 100 кг/м3, предпочтительно составляющей в диапазоне 30-60 кг/м3, при этом указанный способ включает в себя взаимодействие при значении ISO-показателя, составляющем в диапазоне 95-125, между:9. A method of forming an elastic polyurethane foam, characterized by a free-lift density value of less than 100 kg / m 3 , preferably in the range of 30-60 kg / m 3 , said method including interaction with an ISO value of range 95-125, between: - полиизоцианатной композицией;- polyisocyanate composition; - реакционноспособной по отношению к изоцианатам композицией;- reactive with respect to isocyanates composition; - наноразмерными полимочевинными частицами и/или дисперсией наноразмерных частиц, полученными в соответствии с любым из - nanosized polyurea particles and / or dispersion of nanosized particles obtained in accordance with any of пп. 1-8,p. 1-8, - вспенивающим агентом,- blowing agent - катализатором, а также,- a catalyst, as well as - необязательно, добавками, такими как ингибиторы горения, поверхностно-активные вещества,- optionally, additives, such as combustion inhibitors, surfactants, таким образом, что содержание (масс %) полимочевинных частиц в составе получаемого эластичного пенопласта составляет в диапазоне от минимально 1% до максимально 10% масс, предпочтительно составляет в диапазоне 1-5% масс в расчете на общий вес эластичного пенопласта.so that the content (mass%) of polyurea particles in the composition of the obtained elastic foam is in the range from a minimum of 1% to a maximum of 10% of the mass, preferably in the range of 1-5% of the mass, based on the total weight of the elastic foam. 10. Способ образования эластичного полиуретанового эластомера, характеризующегося величиной плотности, составляющей в диапазоне 200-1200 кг/м3, при этом указываемый способ включает в себя взаимодействие при значении ISO-показателя в диапазоне 95-125, между:10. The method of formation of an elastic polyurethane elastomer, characterized by a density value of component in the range of 200-1200 kg / m 3 , while this method includes the interaction when the value of the ISO-indicator in the range of 95-125, between: - полиизоцианатной композицией;- polyisocyanate composition; - реакционноспособной по отношению к изоцианатам композицией;- reactive with respect to isocyanates composition; - наноразмерными полимочевинными частицами и/или дисперсией наноразмерных частиц, полученными в соответствии с любым из пп. 1-8,- nanosized polyurea particles and / or dispersion of nanosized particles obtained in accordance with any of paragraphs. 1-8, - необязательно, вспенивающим агентом,- optionally, a blowing agent, - катализаторами, а также,- catalysts, as well as - необязательно, добавками, такими как ингибиторы горения, поверхностно-активные вещества,- optionally, additives, such as combustion inhibitors, surfactants, таким образом, что содержание (масс %) полимочевинных частиц в составе получаемого эластомера составляет в диапазоне от минимально 1% до максимально 10% масс, предпочтительно составляет в диапазоне 0,5-10% масс, более предпочтительно составляет в диапазоне 1-7% масс в расчете на общий вес эластомера.so that the content (mass%) of polyurea particles in the composition of the obtained elastomer is in the range from a minimum of 1% to a maximum of 10% of the mass, preferably is in the range of 0.5-10% of the mass, more preferably is in the range of 1-7% of the mass calculated on the total weight of the elastomer. 11. Применение наноразмерных полимочевинных частиц и/или дисперсии полимочевинных частиц, изготовленных в соответствии с любым из пп. 1-8, в целях увеличения твердости при сжатии, предела прочности на разрыв и предела прочности при растяжении эластичного пенополиуретана, характеризующегося величиной 11. The use of nanosized polyurea particles and / or dispersion of polyurea particles made in accordance with any one of paragraphs. 1-8, in order to increase the compressive strength, tensile strength and tensile strength of elastic polyurethane foam, characterized by плотности при свободном подъеме менее 100 кг/м3, составляющей в диапазоне 30-60 кг/м3.density with free rise of less than 100 kg / m 3 , component in the range of 30-60 kg / m 3 . 12. Применение наноразмерных полимочевинных частиц и/или дисперсии полимочевинных частиц, изготовленных в соответствии с любым из пп. 1-8, для увеличения предела прочности на разрыв, а также величины модуля упругости при растяжении (растягивающее напряжение) полиуретановых эластомеров, характеризующихся величиной плотности в диапазоне 200-1200 кг/м3. 12. The use of nanosized polyurea particles and / or dispersion of polyurea particles made in accordance with any one of paragraphs. 1-8, to increase the tensile strength, as well as the magnitude of the tensile modulus (tensile stress) of polyurethane elastomers, characterized by a density in the range of 200-1200 kg / m 3 .
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